Phosphorus oxychloride → 7-Bromo-1-chloro-6-methoxyisoquinoline

HRID 2045703노트

반응식

HRID 2045703 반응식
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][NH:8][C:9]2=O)=[CH:4][C:3]=1[O:13][CH3:14].P(Cl)(Cl)([Cl:17])=O>>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N:8]=[C:9]2[Cl:17])=[CH:4][C:3]=1[O:13][CH3:14]

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 580051257-Bromo-6-methoxy-1(2H)-isoquinolinone

생성물 1

HCID 595711467-Bromo-1-chloro-6-methoxyisoquinoline

실험 절차

A mixture of the product from step 2 (7-bromo-6-methoxyisoquinolin-1(2H)-one) (4.7 g, 18.5 mmol) in phosphorus oxychloride (30 mL) was heated to reflux. After 2 h, the mixture was cooled to RT; the volatiles were evaporated, and the residue was partitioned between 3M NaOH and DCM. The organic phase was dried over Na2SO4; solvent was evaporated; and the solid was triturated with Et2O (20 mL) and filtered to give a solid (3.75 g). LRMS ESI+ (M+H)+274.0.

후처리

  1. temperaturewas heated to reflux
  2. customthe volatiles were evaporated
  3. customthe residue was partitioned between 3M NaOH and DCM
  4. dry with materialThe organic phase was dried over Na2SO4
  5. customsolvent was evaporated
  6. customand the solid was triturated with Et2O (20 mL)
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-00308b1052d444d38b285009291689d4
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08591878B2

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